CN105060347B - Method for synthesizing ultrathin molybdenum disulfide nanocrystals - Google Patents
Method for synthesizing ultrathin molybdenum disulfide nanocrystals Download PDFInfo
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Abstract
The invention discloses a method for synthesizing ultrathin molybdenum disulfide nanocrystals and belongs to the technical field of inorganic material preparation processes. According to the method, a molybdenum-containing inorganic salt and a sulfur-containing compound or sulfur powder are used as raw materials and have a reaction at the temperature of 160-300 DEG C for 30-120 min in a long-chain amine solvent and a long-chain fatty acid surfactant, experiment parameters such as the reactant molar ratio, the reactant concentration, the reaction temperature, the reaction time and the like are controlled, molybdenum disulfide nanocrystals which are well crystallized and have a few atomic layers (1-5 layers) are formed and can be well dispersed in a nonpolar solvent or base oil, and stable lubricating oil is formed. According to the method, raw materials are cheap and easy to obtain, the reaction time is short, the yield is high, instruments and equipment are simple, operation is convenient, safe and reliable, process repeatability is good, product quality is stable, and the method is suitable for industrial enlarged production.
Description
Technical field
The present invention relates to a kind of method synthesizing ultra-thin molybdenum disulfide nano crystalline substance, belong to inorganic material preparation process technical field.
Background technology
Molybdenum bisuphide is used for lubricating oil and grease, is the antifriction of excellent performance, wear-resistant and extreme pressure material.Molybdenum bisuphide kollag
Can be dispersed in grease, lubricating oil, water and organic solvent (such as 0.5%～85%) in certain proportion, it is also possible to be used alone,
Coating can also be modulated into various resins and be used as each metalloid, alloy component, the surface conditioning agent of ceramic material.Over half a century with
Coming, molybdenum bisuphide obtains extensively application at the mechanical lubrication such as bearing, gear, industry manufacture view.Low for solving energy utilization rate
Present situation, based on the greasy property that molybdenum bisuphide is excellent, domestic and international scientific research personnel is carrying out the synthesis of novel molybdenum bisuphide always and application is ground
Study carefully.There is the molybdenum bisuphide of a few atomic in recent years owing to it is in utilization of energy, as electrochemistry produces hydrogen, photochemical catalyzing, lithium from
The fields such as sub-battery receive the extensive concern of researcher.
Production has the ultra-thin molybdenum bisuphide of a few atomic (1-5 layer) and is presently mainly stripping method and chemical vapour deposition technique.Wherein
Stripping method is broadly divided into mechanical stripping and chemical stripping.These methods are relatively costly, and operation sequence is complicated, the longest, and energy consumption is high, no
Easily it is amplified commercial production.In this year, some research institutions have attempted utilizing wet chemical method to go to synthesize and have the two of a few atomic
Molybdenum sulfide nanocrystalline (Chemistry of Materials, volume 23,3879-3885 page, 2011).But the method needs temperature pole
Height, and the molybdenum bisuphide crystallization of synthesis is poor, yields poorly, is unfavorable for promoting the use of.So in order to realize there is the super of a few atomic
Thin molybdenum bisuphide, in the commercial Application as fields such as lube oil additives, research one simple process, constant product quality, time-consumingly lacks,
Economical, it is easy to the preparation method of batch production is a challenge of chemical science and technology field face.
Summary of the invention
It is an object of the invention to provide the synthetic method of a kind of ultra-thin molybdenum disulfide nano crystalline substance with a few atomic, the method uses
Raw material cheap and easy to get, utilizes simple approach, it is possible to synthesize in a large number, to fill up the ultra-thin molybdenum disulfide nano with a few atomic
Blank in terms of brilliant simple preparation.Owing to the method is prone to amplify, regulation and control are convenient, excellent product performance, and Modulatory character is strong, will be in profit
The fields such as oil additive have wide market prospect.
Technical scheme is as follows:
A kind of method synthesizing a few atomic molybdenum disulfide nano crystalline substance, it is characterised in that the method is carried out as follows:
1) in long-chain amine solvent, it is initially charged long-chain fat acid additive, adds containing molybdenum inorganic salt and sulfur-containing compound, two kinds of chemical combination
The mol ratio of thing is 0.1～10:1, and the total mass concentration of two kinds of compounds is 0.01～2.0 gram/ml solvent；
2) range of reaction temperature is 160～300 DEG C, and reaction time range is 30～120 minutes；
3) by products therefrom washing with alcohol, molybdenum disulfide nano is directly obtained after being scattered in hexamethylene preservation, or drying brilliant
Powder.
In technique scheme, described long-chain amine solvent preferably employ the one in oleyl amine, 18-amine., cetylamine and tetradecy lamine or
Several mixed solvents.
In technique scheme, described long-chain fat acid additive preferably employs oleic acid or the one of enuatrol or mixed solvent.
In technique scheme, described molybdenum salt preferably employs ammonium molybdate or sodium molybdate；Described sulfur-containing compound preferably employs thiourea
Or sulfur powder simple substance.
The present invention compared with prior art, has the following advantages and salience effect: the present invention uses inorganic salt to be raw material, and long-chain
Amine such as oleyl amine, 18-amine., cetylamine or tetradecy lamine are solvent, use simple wet chemical method to prepare and have a few atomic
Molybdenum disulfide nano is brilliant.Product size is less, good dispersion, the atom number of plies from 1 layer to 5 layer, and well-crystallized.Compared to other
The method of preparation a few atomic molybdenum bisuphide, the most important advantage of the method is exactly with low cost, can amplify and carry out commercial production,
The method raw material is cheap and easy to get simultaneously, and technique is comparatively simple, produces and is prone to amplify, and product has the most outstanding oil-soluble, and makes
The standby ultra-thin molybdenum disulfide nano obtained can directly be scattered in lube base oil, and technique is the simplest.In a word, the present invention provides
A kind of alloy that synthesizes has the simple method that the molybdenum disulfide nano of a few atomic is brilliant, is very suitable for industrialization and amplifies raw
Produce, there is the most wide application prospect.
Accompanying drawing explanation
Fig. 1 is the x-ray diffractogram of powder that series has the molybdenum disulfide nano crystalline substance of a few atomic.
Fig. 2 is the transmission electron microscope figure of the molybdenum disulfide nano crystalline substance with a few atomic.
Detailed description of the invention
The present invention is described further with embodiment below in conjunction with the accompanying drawings
A kind of method synthesizing a few atomic molybdenum disulfide nano crystalline substance that the present invention provides, the method is carried out as follows:
1) in long-chain amine solvent, it is initially charged long-chain fat acid additive, adds containing molybdenum inorganic salt and sulfur-containing compound, two kinds of chemical combination
The mol ratio of thing is 0.1～10:1, and the total mass concentration of two kinds of compounds is generally 0.01～2.0 gram/ml solvent；Described sulfur-containing compound
Preferably employ thiourea or sulfur powder simple substance；Described molybdenum salt preferably employs ammonium molybdate or sodium molybdate；Described long-chain amine solvent is preferably adopted
With the mixed solvent of one or more in oleyl amine, 18-amine., cetylamine and tetradecy lamine；Described long-chain fat acid additive is preferably adopted
With oleic acid or the one of enuatrol or mixed solvent；
2) range of reaction temperature is 160～300 DEG C, and reaction time range is 30～120 minutes；
3) by products therefrom washing with alcohol, molybdenum disulfide nano is directly obtained after being scattered in hexamethylene preservation, or drying brilliant
Powder.
Embodiment 1
Take 10ml oleyl amine and 1ml oleic acid be heated to 160 DEG C, wherein put into mol ratio be 1:10, gross mass be the molybdic acid of 0.1g
Ammonium and thiourea, react 30 minutes, precipitates with washing with alcohol gained, be dried at 40 DEG C after pouring out oleyl amine and oleic acid mixed solvent, can
Brilliant to obtain having the ultra-thin molybdenum disulfide nano of a few atomic.Products obtained therefrom has all carried out table with XRD and transmission electron microscope
Levy.Its powder X-ray diffraction spectrogram is as shown in Figure 1.Its transmission electron microscope photo as shown in Figure 2, the MoS wherein synthesized2
Major part is the MoS of 1-5 atomic layer2Nanocrystalline.
Embodiment 2
Take 10ml oleyl amine and 1g enuatrol be heated to 300 DEG C, wherein put into mol ratio be 1:5, gross mass be the ammonium molybdate of 20g
And thiourea, react 120 minutes, precipitate with washing with alcohol gained after pouring out oleyl amine, be dried at 40 DEG C, can obtain that there is minority
The ultra-thin molybdenum disulfide nano of atomic layer is brilliant.Products obtained therefrom is all characterized with XRD and transmission electron microscope.
Embodiment 3
Take 10ml 18-amine. and 5ml oleic acid be heated to 240 DEG C, wherein put into mol ratio be 5:2, gross mass be the molybdic acid of 5g
Ammonium and thiourea, react 60 minutes, precipitates with washing with alcohol gained, be dried at 40 DEG C after pouring out oleyl amine and oleic acid mixed solvent, can
Brilliant to obtain having the ultra-thin molybdenum disulfide nano of a few atomic.Products obtained therefrom has all carried out table with XRD and transmission electron microscope
Levy.
Embodiment 4
Take 10ml oleyl amine and 10ml oleic acid be heated to 250 DEG C, wherein put into mol ratio be 1:2, gross mass be the sodium molybdate of 2g
And thiourea, react 30 minutes, precipitate with washing with alcohol gained after pouring out oleyl amine and oleic acid mixed solvent, be dried at 40 DEG C, permissible
The ultra-thin molybdenum disulfide nano obtaining having a few atomic is brilliant.Products obtained therefrom is all characterized with XRD and transmission electron microscope.
Embodiment 5
Take 10ml oleyl amine and 1ml oleic acid be heated to 250 DEG C, wherein put into mol ratio be 1:2, gross mass be the ammonium molybdate of 0.5g
And thiourea, react 40 minutes, precipitate with washing with alcohol gained after pouring out oleyl amine and oleic acid mixed solvent, be dried at 40 DEG C, permissible
The ultra-thin molybdenum disulfide nano obtaining having a few atomic is brilliant.Products obtained therefrom is all characterized with XRD and transmission electron microscope.
Embodiment 6
Take 10ml oleyl amine and 0.5g enuatrol be heated to 250 DEG C, wherein put into mol ratio be 1:2, gross mass be the molybdic acid of 10g
Ammonium and thiourea, react 30 minutes, precipitates with washing with alcohol gained, be dried, can obtain having minority at 40 DEG C after pouring out oleyl amine
The ultra-thin molybdenum disulfide nano of atomic layer is brilliant.Products obtained therefrom is all characterized with XRD and transmission electron microscope.
Claims (4)
1. one kind synthesizes the method that ultra-thin molybdenum disulfide nano is brilliant, it is characterised in that the method is carried out as follows:
1) being initially charged long-chain fat acid additive in long-chain amine solvent, add molybdenum salt and sulfur-containing compound, range of reaction temperature is 160～300 DEG C, and reaction time range is 30～120 minutes；The mol ratio of molybdenum salt and sulfur-containing compound is 0.1～10:1, and both total mass concentrations are 0.01～2.0 gram/mL；
2) by products therefrom washing with alcohol, the molybdenum disulfide nano crystalline flour end that the atom number of plies is from 1 layer to 5 layer after being scattered in hexamethylene preservation, or drying, is directly obtained.
2. according to a kind of method synthesizing ultra-thin molybdenum disulfide nano crystalline substance described in claim 1, it is characterised in that: long-chain amine solvent uses the mixed solvent of one or more in oleyl amine, 18-amine., cetylamine and tetradecy lamine.
3. according to a kind of method synthesizing ultra-thin molybdenum disulfide nano crystalline substance described in claim 1, it is characterised in that: long-chain fat acid additive uses oleic acid or the one of enuatrol or mixed solvent.
4. according to a kind of method synthesizing ultra-thin molybdenum disulfide nano crystalline substance described in claim 1,2 or 3, it is characterised in that: described molybdenum salt uses ammonium molybdate or sodium molybdate；Described sulfur-containing compound uses thiourea or sulfur powder simple substance.
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| US10883046B2 (en) * | 2017-02-02 | 2021-01-05 | Nanoco 2D Materials Limited | Synthesis of luminescent 2D layered materials using an amine-met al complex and a slow sulfur-releasing precursor |
| CN106893323A (en) * | 2017-03-03 | 2017-06-27 | 江苏大学 | A kind of ultra-thin molybdenum disulfide nano sheet/Self-lubrication composite material of polyimide and preparation method thereof |
| CN108929742B (en) * | 2018-08-31 | 2020-12-15 | 清华大学 | Nano molybdenum disulfide lubricating oil and preparation method thereof |
| CN109110816B (en) * | 2018-10-30 | 2020-09-11 | 中国石油大学(华东) | Synthetic method of oil-soluble molybdenum disulfide |
| CN109943310B (en) * | 2019-04-02 | 2022-05-24 | 侯吉瑞 | Modified MoS2Nano material and preparation method thereof |
| CN111378928B (en) * | 2020-04-22 | 2021-06-29 | 中国科学院兰州化学物理研究所 | Nanocrystalline MoS2Solid lubricating film and preparation method and application thereof |
| CN111925668A (en) * | 2020-07-14 | 2020-11-13 | 申雨润滑科技有限公司 | Intercalation inlaid coated oil-soluble molybdenum-based lubricating oil additive and preparation method thereof |
| CN114570937B (en) * | 2022-03-04 | 2024-03-29 | 北京市科学技术研究院分析测试研究所(北京市理化分析测试中心) | Synthesis method of superfine monodisperse nano Ag |
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